This work highlights testing the polymer nanocomposite for hydrogen gas production from wastewater (sewage water). The in-situ polymerization technique is used to prepare polypyrrole (PPy) and PPy/NiO x nanocomposite films on a glass substrate. The film's ability to generate hydrogen from sewage water is then evaluated. The XRD and XPS confirmed the formation of two types of NiO X : NiO and Ni 2 O 3 . The optical property of the composite is greater than the polymer under the insertion of NiO x as a core for the polymer coating shell, in which the band gap values are 2.25 and 1.81 eV, respectively. The TEM confirmed the PPy/NiO x core-shell formation, in which the polymer shell (20 nm) coated the NiO X core (170 nm). The electrochemical testing for H 2 gas production is carried out through a three-electrode cell. The effect of light on/off, wavelengths, and temperature on the H 2 production is applied. Under